Manufacture of by-products from distillery-slop.



ALADAR von LAszLoFFY, or PEORIA. ILLINOIS.

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MANUFACTURE OF BY-PRODUCTS FROM DISTILLERY-SLOP.

No Drawin g. Original application filed January 30, 1911,

Specification of Letters Patent.

Patented July 27, 1915.

Serial No. 605,611. Divided and this application filed February 26. 1912. Serial No. 679,990.

To all whom it may con cern Be it known that .T, Arno/in vox Lisz- LOFFY, citizen of the llnited States, residing at Peoria, in the county of Peoria and State of Illinois, have invented certain-11c and useful Improvements in Manufacture of By- Products from Distillery-Slop; and I do hereby declare that the following is a full, clear, and exact description of the invention, which will art to which it appertains to make and use the same.

, This invention relates to a process of recovering lay-products from distillery-slop.

The object of the invention is to provide a process of recovering from distillery-slop a plurality of valuable products by first extracting from the slop a mixture containing the by-products in a concentrated state, and afterward se oarating the several by-products container in this mixture from one another.

The present application is divided from my pending application for the manufacture of by-products from. distillery slop Serial Number 605,611, filed January 30, 1911, in which has been described the manner of extracting from distillery slop a mixture in which is contained lactic acid, succinic acid and glycerin, and also fat, if the slop conlains it. by treating the concentrated slop uith ethyl-alcohol. methyl alcohol, higher alcohols, or mixtures of the same with ethyl ether. fusel oil. chlopolorm, tetrachlorid of carbon, or other rnxtures in whichalcohol predominates.

While the just waitioned processembraces the methods of obtaining the mixture of byproducts, the present process represents one of the methods of singling out the individual components of this mixture.

The following, which is the preferred mode-of practising the present invention, explains the manner of procedure. The distillery slop having been concentrated preferably to a syrupy consistency as described in the application above referred to and treated with an alcoholic solvent gives an insoluble residue containing the albuminous gummy and other substances of the a solution containing the lactic acid, succinic acid, glycerin and fat in a concentrated state. The solution concentrated by evaporating the solvent, and this mixture, hereinitlfter referred to as the mixture. of

enable others skilled in the thoroughly slop, and

byproducts, is further separated into components. 'l he singling out of the fat, lactic acid. succmic acid, and glycerin is accom-v plishcd in the present processby the use of solvents which can only dissolve certain of the substances. That is to say, the substances contained in the mixture are each acted on according to its degree of solubility in the solvent used. The action on the mixture of by-products is brought about by in any suitable receptacle. The fat may be eliminated at the beginning of the treatment since it is insoluble in the other substances present in the mixture and can, therefore, be easily separated from the same by reason of its difierence in specific gravity. For instance, it may be allowed to rise to and accumulate upon the surface of the mixture and may then be skimmed off, or, it may be removed in any later stage of the process if desired. The next step is the separation of the organic acids from the remaining mixture of other by-products. This separation is effected by treating the mixture of byproducts with ethyl-ether, for example, as the solvent. This solvent dissolves the lac tie and succinic acids and but very little of the glycerin, which latter remains in the residue. The ethyl-ether does not easily penetrate and act on the mixture of byproducts since the character and behavior of the latter toward it is dominated by the glycerin, water and impurities which are almost insoluble in ether. Since the mixture of by-products and the ether do not easily mix, but rather repel each other, I may bring about a more intimate contact between them by agitation. or the mixture of by-prmlncts and solvent may be spread over a large surface, as for example. upon and tlnrough an absorbent material for instance gypsum. But other methods may be resorted to. to bring about the dissolving action of the ether on the mixture of byproducts in such a. way that the ether can reach finely divided portions of the said mixture.

'Ihe solution resulting from the treatment of the mixture of by-products with ether contains the lactic and succinic acids and fat, if that substance has not already been eliminated from the mixture before the treatment with ether as before stated. Now, by concentrating the solution as, for inmixing the solvent with the same tains the lactic and succinic acids of a high grade of purity. I have found that owing to this great purity the succinic acid will crystallize, if the concentrated solution is allowed to stand. The crystals can be easily separated from the solution which contains the lactic acid either by settling, filtering or by the use of a centrifugal machine. I thus .utilize the simple crystallizing process for the separation of the lactic and succinic acids from one another.

Having described the treatment of the etheric solution, that of the residue containing the glycerin will now be explained. The purity of the glycerin contained in the residue depends on the character of the slop and the character of the solvent used for obtaining the original mixture of by-products. Any impurities may be eliminated therefrom by any of the known processes, for instance, by treatment with bone-coal, distillation,'treatment with lime, sulfuric acid and like methods.

The above described process of singling out lactic acid, succinic acid, glycerin and fat can be used not only in connection with the method mentioned of extracting a mixture of by-products, but, of course, can be used also to separate the components of a mixture of by-products obtained by other processes. Besides the use with ethyl-ether the process can be practisedwith fusel oil, mixtures of both or such other solvents as are capable of dissolving lactic and succinic acids but which dissolve very little or no glycerin, such solvents of whatever nature being considered equivalents. I have found,

however, that ethyl-ether is .the most advantageous solvent for carrying out this process and therefore it is used with preference, but

vent capable of dissolving the organic acids' of the slop and capable also of repelling glycerin, separating the solution resulting from this treatment from the. insoluble part,

concentrating the solution by eliminating the solvent to liberate the fat, and separating the fat from the remaining solution.

2. In the process of recovering lactic and succinic acid from distillery slop from which the gummyand albuminous substances have been eliminated, the steps which. consist in treating such a distillery slop with a solvent capable of dissolving the organic acids therein and capable also of repelling glycerin, separating the solution resulting from this treatment from the insoluble part, con

centrating' the solution by eliminating the solvent, and accomplishing the separation of the lactic acid contained in the solution from the succinic acid by allowing the succinic acid to crystallize.

In testimony whereof I aflix'my signature, in presenceof two witnesses.

' ALADARjvon-LASZLOFFY.

Witnessesi v EUNICE -M. "Bnoxum,

M. Tnunmw. 

